CN107384109B - High-reliability UV (ultraviolet) curing conformal coating and preparation method thereof - Google Patents
High-reliability UV (ultraviolet) curing conformal coating and preparation method thereof Download PDFInfo
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- CN107384109B CN107384109B CN201710608779.9A CN201710608779A CN107384109B CN 107384109 B CN107384109 B CN 107384109B CN 201710608779 A CN201710608779 A CN 201710608779A CN 107384109 B CN107384109 B CN 107384109B
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- C09D147/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Coating compositions based on derivatives of such polymers
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Abstract
The invention provides a high-reliability UV curing conformal coating which is prepared from the following raw materials in parts by weight: 20-40 parts of epoxidized polybutadiene modified acrylate resin, 30-50 parts of dicyclopentadiene acrylate monomer, 15-25 parts of acrylate monomer containing rigid groups and 1-7 parts of photoinitiator. The high-reliability UV curing conformal coating prepared by the invention introduces two rubber molecular structures of polybutadiene and dicyclopentadiene into macromolecules of the polymer, and the molecular structures have better water resistance and salt fog resistance, so that the defect that the conventional conformal coating is not resistant to salt fog can be solved. In addition, the special epoxidized polybutadiene modified acrylate resin is synthesized, carbon-carbon double bonds in the epoxidized acrylate structure have higher reactivity, and the obtained conformal coating is lower in curing energy and is a high-reliability UV-cured conformal coating with low energy consumption.
Description
Technical Field
The invention belongs to the field of photocuring materials, and relates to a high-reliability UV-cured conformal coating and a preparation method thereof, which are suitable for the application requirement of high-end circuit board protection.
Background
Conformal coating is a very thin protective material applied to a Printed Circuit Board (PCB) to which the connector components have been soldered. The anti-corrosion and anti-pollution circuit board can enhance the moisture-proof and anti-pollution capacity of electronic circuits and components, prevent welding spots and conductors from being corroded, play a role in shielding and eliminating electromagnetic interference and preventing short circuit of the circuits, and improve the insulating property of the circuit board. In addition, the coating protective film is also beneficial to the friction resistance and the solvent resistance of circuits and components, can release pressure caused by periodic temperature change, improves the stability of electronic products and prolongs the service life. In addition to use in the electronics industry, conformal coatings have also found wide application in the automotive industry, aerospace industry, defense industry and bioengineering.
The photo-curing coating is also called Ultraviolet (UV) curing coating, is one kind of radiation curing coating, mainly refers to a kind of novel coating which can be rapidly cross-linked and cured to form a film under the irradiation of light, and has been widely used in the coating industry due to the characteristics of high-efficiency coating, environmental friendliness and the like. Compared with solvent-based coatings, the photocureable coating has the characteristics of high curing speed, volatile solvent, energy conservation, low cost, automatic production and the like.
However, the conventional UV-curable conformal coating has disadvantages such as high curing energy, high water absorption, poor low-temperature flexibility, and insufficient salt spray resistance, and the high-reliability UV-curable conformal coating can solve the disadvantages.
Disclosure of Invention
In order to solve the problem that the UV curing conformal coating in the prior art is poor in salt spray resistance and curing energy, the invention provides the high-reliability UV curing conformal coating and the preparation method thereof, so that the conformal coating can meet the requirement of high reliability.
The technical scheme for solving the technical problems is as follows:
a high-reliability UV curing conformal coating is composed of the following raw materials in parts by weight: 20-40 parts of epoxidized polybutadiene modified acrylate resin, 30-50 parts of dicyclopentadiene acrylate monomer, 15-25 parts of acrylate monomer containing rigid groups and 1-7 parts of photoinitiator.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, the epoxidized polybutadiene modified acrylate resin refers to an epoxidized polybutadiene modified acrylate resin having a polybutadiene rubber structure synthesized by using epoxidized polybutadiene and acrylic acid, wherein the epoxidized polybutadiene comprises: epolead PB3600, Epolead PB4700, CAS number: 71342-74-0. The synthesis method of the epoxidized polybutadiene modified acrylate resin comprises the following steps: 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and a catalyst triphenylphosphine (50 ppm) are added into a three-neck flask with a thermometer, the temperature is controlled at 100 ℃ and 120 ℃, and the heating is stopped after the reaction is carried out for 3 hours, so that the epoxidized polybutadiene modified acrylate resin can be obtained.
Further, the dicyclopentadiene acrylate monomers are 512AS (CAS number: 65983-31-5) and 512M (CAS number: 68586-19-6) produced by Hitachi, Japan, and the molecular chain contains the molecular structure of cyclopentadiene.
Further, the rigid group-containing acrylate monomer refers to 4-t-butylcyclohexyl acrylate (CAS: 84100-23-2) and p-t-butylcyclohexyl methacrylate (CAS: 46729-07-1), for example: SR217 and SR218 from SARTOMER, molecular structural formula as follows:
methacrylic acid p-tert-butylcyclohexyl ester
4-tert-butylcyclohexyl acrylate
Further, the photoinitiator is one or a mixture of any more of trade marks 1173 (2-hydroxy-2-methyl-1-phenyl acetone), 184 (1-hydroxycyclohexyl phenyl ketone), 907 (2-methyl-1- (4-methylmercaptophenyl) -2-morpholine-1-one), 369 (2-benzyl-2-dimethylamino-1- (4-morpholine-phenyl) -1-butanone), 819 (bis (2,4, 6-trimethylbenzoyl) phenyl phosphorus oxide), 651(α' -dimethyl benzil ketal), ITX (isopropyl thioxanthone), BP (benzophenone), OMBB (methyl o-benzoylbenzoate), TPO (2,4, 6-trimethylbenzoyl diphenyl phosphorus oxide).
The preparation method of the high-reliability UV curing conformal coating comprises the following steps: weighing 20-40 parts of epoxidized polybutadiene modified acrylate resin, 30-50 parts of dicyclopentadiene acrylate monomer, 15-25 parts of acrylate monomer containing rigid groups and 1-7 parts of photoinitiator, sequentially adding into a stirrer, vacuumizing to the vacuum degree of-0.08-0.05 MPa, stirring for 0.5-2 hours at 500-1000 rpm, uniformly stirring, naturally airing to room temperature, sealing and packaging.
The invention has the beneficial effects that: the high-reliability UV curing conformal coating prepared by the invention introduces two rubber molecular structures of polybutadiene and dicyclopentadiene into macromolecules of the polymer, and the molecular structures have better water resistance and salt fog resistance, so that the defect that the conventional conformal coating is not resistant to salt fog can be solved. In addition, the special epoxidized polybutadiene modified acrylate resin is synthesized, carbon-carbon double bonds in the epoxidized acrylate structure have higher reactivity, and the obtained conformal coating is lower in curing energy and is a high-reliability UV-cured conformal coating with low energy consumption. In addition, the introduced polybutadiene rubber structure has excellent low-temperature flexibility, and the obtained conformal coating has wider use temperature, can withstand the reliability test of high and low temperature impact, and can protect a circuit board to have excellent performance under the severe environment temperature.
Detailed Description
The principles and features of this invention are described below in conjunction with examples which are set forth to illustrate, but are not to be construed to limit the scope of the invention.
Synthetic examples
The synthesis method of the epoxidized polybutadiene modified acrylate resin comprises the following steps: 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and a catalyst triphenylphosphine (50 ppm) are added into a three-neck flask with a thermometer, the temperature is controlled at 100 ℃ and 120 ℃, and the heating is stopped after the reaction is carried out for 3 hours, so that the epoxidized polybutadiene modified acrylate resin can be obtained.
Example 1
Accurately weighing 30g of epoxidized polybutadiene modified acrylate resin; 512AS, 40g, made by Hitachi chemical; SR217, 20g from SARTOMER; photoinitiator 184, 3 g; photoinitiator TPO, 1 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.08 MPa, stirring at 500 rpm for 2 hours, uniformly stirring, naturally airing to room temperature to obtain the high-reliability UV curing conformal coating, and sealing and packaging.
Example 2
Accurately weighing 40g of epoxidized polybutadiene modified acrylate resin; 512M, 30g of Hitachi chemical; SR217, 18g from SARTOMER; photoinitiator 184, 1 g; photoinitiator 1173, 1 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.05 MPa, stirring at 750 rpm for 1 hour, uniformly stirring, naturally airing to room temperature to obtain the high-reliability UV curing conformal coating, and sealing and packaging.
Example 3
Accurately weighing 20g of epoxidized polybutadiene modified acrylate resin; 512AS, 50g, made by Hitachi chemical; SR218,25g from SARTOMER; photoinitiator 1173: 3g of the total weight of the mixture; photoinitiator 819: 2g, sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing until the vacuum degree is-0.06 MPa, stirring at 700 revolutions per minute for 1.5 hours uniformly, naturally airing to room temperature to obtain the high-reliability UV curing conformal coating, and sealing and packaging.
Example 4
Accurately weighing 35g of epoxidized polybutadiene modified acrylate resin; 512M, 40g of Hitachi chemical; SR218,25g from SARTOMER; photoinitiator 184, 3 g; photoinitiator TPO, 1 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.07 MPa, stirring at 800 rpm for 1 hour, uniformly stirring, naturally airing to room temperature to obtain the high-reliability UV curing conformal coating, and sealing and packaging.
Example 5
Accurately weighing 25g of epoxidized polybutadiene modified acrylate resin; 512AS, 45g, by Hitachi chemical; SR217, 25g from SARTOMER company, 1173, 3g of photoinitiator; photoinitiator TPO, 4 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.08 MPa, stirring at 1000 rpm for 0.5 hour, uniformly stirring, naturally airing to room temperature to obtain the high-reliability UV curing conformal coating, and sealing and packaging.
Comparative example 1
Accurately weighing 30g of CN8881 (bifunctional, polyester type) of Saedoma; IBOA, 60 g; HEA, 10 g; photoinitiator 184, 3 g; photoinitiator TPO, 1 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.08 MPa, stirring at 500 rpm for 2 hours, uniformly stirring, naturally airing to room temperature to obtain the UV-cured conformal coating, and sealing and packaging.
Comparative example 2
The following raw materials, 5220 (bifunctional, polyether type), 35g, from taiwan chang corporation were weighed accurately; THFA, 41 g; IBOA, 15 g; photoinitiator 1173, 3 g; photoinitiator TPO, 1 g; sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing to the vacuum degree of-0.05 MPa, stirring at 750 rpm for 1 hour, uniformly stirring, naturally airing to room temperature to obtain the UV curing conformal coating, and sealing and packaging.
The performance of a highly reliable UV-curable conformal coating of the present invention was tested by the following test.
Test examples
Testing the salt spray resistance: tested according to GB/T10125-1997 standard.
Water absorption test: tested according to GB/T1034-1998 standard, 100 ℃ boiling water for 2 h.
The test results are shown in table 1:
TABLE 1 comparative test results of samples prepared in examples 1-5 with conventional UV-curable conformal coating materials
| Test specimen | Curing energy | Water absorption rate | Salt spray resistance | Low temperature flexibility |
| Sample of example 1 | 800mJ/cm2 | 0.4% | Excellent and no rust spot | Is excellent in |
| Sample of example 2 | 800mJ/cm2 | 0.5% | Excellent and no rust spot | Is excellent in |
| Sample of example 3 | 900mJ/cm2 | 0.6% | Excellent and no rust spot | Is excellent in |
| Sample of example 4 | 800mJ/cm2 | 0.5% | Excellent and no rust spot | Is excellent in |
| Sample of example 5 | 850mJ/cm2 | 0.6% | Excellent and no rust spot | Is excellent in |
| Sample of comparative example 1 | 1200mJ/cm2 | 1.2% | Generally, there are rust spots | Crispness at-40 ° |
| Sample of comparative example 2 | 1300mJ/cm2 | 1.0% | Generally, there are rust spots | Crispness at-40 ° |
From the results, compared with the existing common UV curing conformal coating, the high-reliability UV curing conformal coating has the advantages of good salt spray resistance, lower curing energy and better low-temperature flexibility.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (5)
1. A high-reliability UV-curing conformal coating is characterized by comprising the following preparation methods:
1) synthesis of epoxidized polybutadiene modified acrylate resin: adding 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and 50ppm of triphenylphosphine serving as a catalyst into a three-neck flask with a thermometer, controlling the temperature at 100 ℃ and 120 ℃, and stopping heating after reacting for 3 hours to obtain epoxidized polybutadiene modified acrylate resin;
2) 30g of epoxidized polybutadiene modified acrylate resin; 512AS, 40g, made by Hitachi chemical; SR217, 20g from SARTOMER; 3g of photoinitiator 1-hydroxycyclohexyl benzophenone; photoinitiator 2,4, 6-trimethylbenzoyldiphenylphosphine oxide, 1 g; the components are sequentially added into a double-planetary power mixing stirrer, the mixture is vacuumized until the vacuum degree is-0.08 MPa, stirred for 2 hours at 500 revolutions per minute and uniformly stirred, and naturally aired to room temperature, so that the high-reliability UV curing conformal coating is obtained.
2. A high-reliability UV-curing conformal coating is characterized by comprising the following preparation methods:
1) synthesis of epoxidized polybutadiene modified acrylate resin: adding 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and 50ppm of triphenylphosphine serving as a catalyst into a three-neck flask with a thermometer, controlling the temperature at 100 ℃ and 120 ℃, and stopping heating after reacting for 3 hours to obtain epoxidized polybutadiene modified acrylate resin;
2) 40g of epoxidized polybutadiene modified acrylate resin; 512M, 30g of Hitachi chemical; SR217, 18g from SARTOMER; 1g of photoinitiator 1-hydroxycyclohexyl benzophenone; photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone, 1 g; the components are sequentially added into a double-planetary power mixing stirrer, the mixture is vacuumized until the vacuum degree is-0.05 MPa, stirred for 1 hour at 750 revolutions per minute, stirred uniformly and naturally aired to room temperature, and the high-reliability UV curing conformal coating is obtained.
3. A high-reliability UV-curing conformal coating is characterized by comprising the following preparation methods:
1) synthesis of epoxidized polybutadiene modified acrylate resin: adding 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and 50ppm of triphenylphosphine serving as a catalyst into a three-neck flask with a thermometer, controlling the temperature at 100 ℃ and 120 ℃, and stopping heating after reacting for 3 hours to obtain epoxidized polybutadiene modified acrylate resin;
2) 20g of epoxidized polybutadiene modified acrylate resin; 512AS, 50g, made by Hitachi chemical; SR218,25g from SARTOMER; photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone: 3g of the total weight of the mixture; photoinitiator bis (2,4, 6-trimethylbenzoyl) phenylphosphinate oxide: 2g, sequentially adding the components into a double-planetary power mixing stirrer, vacuumizing until the vacuum degree is-0.06 MPa, stirring at 700 revolutions per minute for 1.5 hours uniformly, and naturally airing to room temperature to obtain the high-reliability UV curing conformal coating.
4. A high-reliability UV-curing conformal coating is characterized by comprising the following preparation methods:
1) synthesis of epoxidized polybutadiene modified acrylate resin: adding 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and 50ppm of triphenylphosphine serving as a catalyst into a three-neck flask with a thermometer, controlling the temperature at 100 ℃ and 120 ℃, and stopping heating after reacting for 3 hours to obtain epoxidized polybutadiene modified acrylate resin;
2) 35g of epoxidized polybutadiene-modified acrylate resin; 512M, 40g of Hitachi chemical; SR218,25g from SARTOMER; 3g of photoinitiator 1-hydroxycyclohexyl benzophenone; photoinitiator 2,4, 6-trimethylbenzoyldiphenylphosphine oxide, 1 g; the components are sequentially added into a double-planetary power mixing stirrer, the mixture is vacuumized until the vacuum degree is-0.07 MPa, stirred for 1 hour at 800 revolutions per minute and uniformly stirred, and naturally aired to room temperature, so that the high-reliability UV curing conformal coating is obtained.
5. A high-reliability UV-curing conformal coating is characterized by comprising the following preparation methods:
1) synthesis of epoxidized polybutadiene modified acrylate resin: adding 1 mol of epoxidized polybutadiene, 2 mol of acrylic acid and 50ppm of triphenylphosphine serving as a catalyst into a three-neck flask with a thermometer, controlling the temperature at 100 ℃ and 120 ℃, and stopping heating after reacting for 3 hours to obtain epoxidized polybutadiene modified acrylate resin;
2) 25g of epoxidized polybutadiene-modified acrylate resin; 512AS, 45g, by Hitachi chemical; SR217 from SARTOMER corporation, 25g, photoinitiator 2-hydroxy-2-methyl-1-phenyl acetone, 3 g; photoinitiator 2,4, 6-trimethylbenzoyldiphenylphosphine oxide, 4 g; the components are sequentially added into a double-planetary power mixing stirrer, the mixture is vacuumized until the vacuum degree is-0.08 MPa, stirred for 0.5 hour at 1000 revolutions per minute and uniformly stirred, and naturally aired to room temperature, so that the high-reliability UV curing conformal coating is obtained.
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| CN109957368A (en) * | 2017-12-22 | 2019-07-02 | 比亚迪股份有限公司 | A kind of LED-UV solidification Optical adhesive composition, preparation method and its solidify coating |
| CN109111771A (en) * | 2018-05-31 | 2019-01-01 | 烟台德邦科技有限公司 | A kind of moisture cured high reliability UV conformal coating and preparation method thereof |
| CN116162431B (en) * | 2022-12-30 | 2024-06-14 | 烟台德邦科技股份有限公司 | Hybrid curing damp-heat resistant adhesive and preparation method thereof |
Citations (4)
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|---|---|---|---|---|
| JPS6155807A (en) * | 1984-08-28 | 1986-03-20 | 日立化成工業株式会社 | Thermosetting resin composition for film capacitor |
| JP2005062451A (en) * | 2003-08-12 | 2005-03-10 | Kyocera Chemical Corp | Photosensitive thermosetting resin composition |
| CN101392152A (en) * | 2008-09-28 | 2009-03-25 | 广东恒大新材料科技有限公司 | Photo-setting adhesive |
| CN103865470A (en) * | 2014-02-12 | 2014-06-18 | 惠晶显示科技（苏州）有限公司 | Light-curing edge sealing adhesive |
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- 2017-07-25 CN CN201710608779.9A patent/CN107384109B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6155807A (en) * | 1984-08-28 | 1986-03-20 | 日立化成工業株式会社 | Thermosetting resin composition for film capacitor |
| JP2005062451A (en) * | 2003-08-12 | 2005-03-10 | Kyocera Chemical Corp | Photosensitive thermosetting resin composition |
| CN101392152A (en) * | 2008-09-28 | 2009-03-25 | 广东恒大新材料科技有限公司 | Photo-setting adhesive |
| CN103865470A (en) * | 2014-02-12 | 2014-06-18 | 惠晶显示科技（苏州）有限公司 | Light-curing edge sealing adhesive |
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